CN101693315A - Molten state lead-free welding flux anti-oxidation reducing agent and preparation process thereof - Google Patents
Molten state lead-free welding flux anti-oxidation reducing agent and preparation process thereof Download PDFInfo
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- CN101693315A CN101693315A CN200910210874A CN200910210874A CN101693315A CN 101693315 A CN101693315 A CN 101693315A CN 200910210874 A CN200910210874 A CN 200910210874A CN 200910210874 A CN200910210874 A CN 200910210874A CN 101693315 A CN101693315 A CN 101693315A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention relates to a molten-state lead-free welding flux anti-oxidation reducing agent and a preparation process thereof, which comprise a reducing agent, an antioxidant and a dispersing accelerating agent. The preparation process includes: placing the weighed reducing agent into a stainless steel container, heating the container until the reducing agent is completely melted into liquid, keeping temperature within 100 DEG C-155 DEG C; then stirring and slowly adding the weighed antioxidant into the container at an even speed, adding the dispersing accelerating agent after stopping heating, and further stirring to obtain the molten-state lead-free welding flux anti-oxidation reducing agent. The molten-state lead-free welding flux anti-oxidation reducing agent has the advantages of apparent anti-oxidation effect, high reducing efficiency, long continuous service time, small smoke, no unpleasant odor, and economical and practical properties.
Description
Technical field
A kind of molten state lead-free welding flux anti-oxidation reducing agent is the pb-free solder tin stove surface that is applied to fusion, can reduce scolder oxidation at high temperature, and the composition that can reduce already oxidised tin, belongs to unleaded electronic product assembling welding technology field.
Background technology
In the electronic product assembling welding process, because solder furnace is under the continuous high temperature heated condition, the lead-free solder surface of fusion can constantly produce the oxidation scruff, swims in the tin liquor surface, and especially the crest solder furnace is under mechanism, oxidation is quickened, a large amount of scruffs drops in the tin oven, has a spot of scruff simultaneously and is the silk ribbon shape again and brings back on the tin crest, has not only influenced the welding quality of product, and wasted a large amount of precious metal tin, increased production cost.Experimental study shows, adopts nitrogen protection technology can significantly reduce scruff in the welding and forms, and helps to improve the wetability of pb-free solder, reduces weld defect.But nitrogen protection will increase equipment investment; require in the wave soldering zone that the content of oxygen is less than 50ppm in the nitrogen; constantly consume nitrogen in the production process again; this has increased production cost again; moreover the not advantage only that adopts that nitrogen protection technology brings aspect welding quality; after topmost shortcoming was welding, the PCB surface tin sweat(ing) increased, and the short circuit phenomenon that causes thus is comparatively outstanding.In order to prevent the molten state lead-free welding flux surface oxidation, save precious metal, guarantee that the pb-free solder quality reduces production costs, adding anti-oxidation reducing substances on the fusion welding surface is the most simple and easy to do method.
The anti-oxidation reducing agent product generally has liquid state, solid-state or crystal powder powder, and existing product all is effective through trying out.But still exist the some shortcomings part.1. percent reduction is low, mostly below 80%.2. service time is short continuously.3. cigarette is big in using, and penetrating odor is arranged.4. on the welding rear board obvious residue is arranged, as not cleaning, insulaion resistance is descended, residue mainly is alkyl phenol ethers surfactant and halogen etc. by analysis.
Summary of the invention
Technical problem to be solved by this invention provides a kind of molten state lead-free welding flux anti-oxidation reducing agent in order to overcome above-mentioned weak point exactly, it is a kind ofly can be used for unleaded wave soldering tin stove, manual immersed solder molten tin bath and component down-lead, wire harness are warded off the high-temp antioxidizing reducing substances of the no slicker solder pot that tin uses.
The present invention is a kind of pulvis of being made by following raw material.Its parts by weight of raw materials proportioning is: reducing agent 8-30, antioxidant 65-90 disperses promoter 1-5.
Preparation method of the present invention may further comprise the steps:
A, take by weighing raw material by above-mentioned composition by weight.
B, elder generation put into rustless steel container to the reducing agent that weighs up, and are heated to and all are fused into liquid, and temperature is remained between 100-155 ℃.
C, the antioxidant that weighs up is slowly at the uniform velocity joined in the liquid of b step preparation while stirring, stop heating after in said temperature, stirring 20-30min.
The material of c step preparation is stirred in d, continuation, when its temperature drops to 30-40 ℃, adds while stirring and disperses promoter, stirs 0.5-1h again and promptly gets product of the present invention.
Molten state lead-free welding flux anti-oxidation reducing agent of the present invention has the high-temp antioxidizing function admirable, and is economical and practical, and to already oxidised scruff percent reduction height, continuous service time is long, the little no bad smell of cigarette, the feature that postwelding wiring board face is clean.
The specific embodiment
Molten state lead-free welding flux anti-oxidation reducing agent of the present invention is the pulvis of being made by following weight portion raw material, and its parts by weight of raw materials proportioning is reducing agent 8-30, and antioxidant 65-90 disperses promoter 1-5.
Described reducing agent is glutaric acid, adipic acid, suberic acid, decanedioic acid, can choose wherein a kind of, two or more composite wantonly.Proportioning arbitrarily between the reducing agent of composite two or more.
Described antioxidant is potassium fluoborate, zinc fluoroborate, tin fluoborate, potassium fluosilicate, zinc fluosilicate, fluosilicic acid tin, sodium tetraborate, can choose wherein two kinds composite wantonly.Proportioning arbitrarily between two kinds of composite antioxidants.
Described dispersion promoter is diethylenetriamines, trien, tetren, optional one or both composite.Composite two kinds are disperseed between promoter proportioning arbitrarily.
A kind of preparation method of molten state lead-free welding flux anti-oxidation reducing agent may further comprise the steps:
A, component takes by weighing above-mentioned various raw material by weight.
B, elder generation put into rustless steel container to the reducing agent that weighs up, and are heated to and all are fused into liquid, and temperature is remained between 100-155 ℃.
C, the antioxidant that weighs up is slowly at the uniform velocity joined in the liquid of b step preparation while stirring, mixing speed 40-60n/min stops heating stirring 20-30min in said temperature after.
The material of c step preparation is stirred in d, continuation, when its temperature drops to 30-40 ℃, adds while stirring and disperses promoter, stirs 0.5-1h again and promptly gets product of the present invention.
The anti-oxidation original hase reason of going back of the present invention is: the fusing point of antioxidant, potassium fluoborate, zinc fluoroborate, tin fluoborate, potassium fluosilicate, zinc fluosilicate, fluosilicic acid tin, sodium tetraborate is more than 400 ℃, when the technological temperature of lead-free solder at 255 ℃ between 265 ℃ the time, antioxidant evenly covers the solder surface of fusion, oxygen in the secluding air contacts with the tin face, has avoided scolder oxidation reaction at high temperature.Reducing agent is glutaric acid, adipic acid, suberic acid, decanedioic acid, and its boiling point under welding temperature, has tin oxide in the reduction lead-free solder that goes round and begins again, purifies scolder all more than 275 ℃
The effect on surface.The organic acid functional gene
On hydroxyl and tin oxide effect, hydrogen atom is replaced by metal, generates the more weak acylate of combination degree, floats over the fusion welding surface, has purified the oxide of metal surface.Tin oxide and organic acid action-reaction are as follows:
N=3,4,6,8 wherein.
The organic acid tin that generates is also unstable, can resolve into organic acid under heated condition, restores tin, and reaction equation is as follows:
Under the situation that has tin oxide to exist, organic acid and tin oxide generate organic acid tin by the reaction of (1) formula again, carry out reduction reaction by (2) formula under heating condition.
In order further to strengthen anti-oxidation performance and to improve reduction effect, the present invention adds a certain proportion of dispersion promoter, disperse the effect of promoter to be: one, to increase the flowability of antioxidant, make its even dispersion cover the solder surface the superiors comprehensively at the melt solder surface.Two, disperseing promoter diethylenetriamines, trien, tetren is the alkaline matter that ammonia odor is arranged, and at high temperature ammonia wherein can resolve into nitrogen and hydrogen, and nitrogen forms the nitrogen protective layer above the melt solder surface, strengthens antioxygenic property.Organic acid tin effect in hydrogen and (2) formula restores simple metal tin and has improved reduction effect.
Through long-term test and use proof, reducing agent of the present invention, the synergy of antioxidant and the triplicity of dispersion promoter makes molten state lead-free welding flux anti-oxidation reducing agent have good anti-oxidation performance, oxidation scruff percent reduction more than 95%, after using 72h continuously under the welding procedure temperature, the proportion of goods damageds of anti-oxidation reducing agent are not more than 30% good adaptability and stability, in the use cigarette little, do not have a bad smell, the no visible residue of the clean light of the wiring board face after the welding.
Specify the present invention with embodiment below:
Embodiment 1
The anti-oxidation reducing agent raw material is formed: glutaric acid 18kg, potassium fluoborate 30kg, tin fluoborate 50kg, trien 2kg.
The preparation method:
Glutaric acid is placed rustless steel container, be heated to and all be fused into liquid, temperature remains on 100 ℃.
Potassium fluoborate, tin fluoborate are slowly at the uniform velocity joined in the prepared liquid, stir 25min down at 100 ℃, mixing speed is 50n/min, stops heating afterwards.
Continue to stir the material of above-mentioned preparation, when its temperature drops to 40 ℃, add trien, stir 0.5h again, promptly get anti-oxidation reducing agent of the present invention.
Embodiment 2
The anti-oxidation reducing agent raw material is formed: suberic acid 2kg, adipic acid 10kg, decanedioic acid 14kg, zinc fluosilicate 31kg, sodium tetraborate 38kg, diethylenetriamines 3kg, trien 2g.
The preparation method:
Suberic acid, adipic acid, decanedioic acid are placed rustless steel container, be heated to and all be fused into liquid, temperature remains on 155 ℃.
Zinc fluoroborate, sodium tetraborate are slowly at the uniform velocity joined in the prepared liquid, stir 30min down at 155 ℃, mixing speed is 60/min, stops heating afterwards.
Continue to stir the material of above-mentioned preparation, when its temperature drops to 30 ℃, add diethylenetriamines, trien, stir 1h again, promptly get anti-oxidation reducing agent of the present invention.
Embodiment 3
Anti-oxidation reducing agent is formed: decanedioic acid 5kg, glutaric acid 3kg, zinc fluoroborate 10kg, fluosilicic acid tin 80kg, tetren 2kg.
The preparation method:
Decanedioic acid, glutaric acid are placed rustless steel container, be heated to and all be fused into liquid, temperature remains on 135 ℃.
Zinc fluoroborate, fluosilicic acid tin are slowly at the uniform velocity joined in the prepared liquid, stir 20min down at 135 ℃, mixing speed 40n/min stops heating afterwards.
Continue to stir the material of above-mentioned preparation, when its temperature drops to 35 ℃, add tetren, stir 1h again, promptly get anti-oxidation reducing agent of the present invention.
Embodiment 4
The anti-oxidation reducing agent raw material is formed: glutaric acid 15kg, suberic acid 10kg, decanedioic acid 51kg, potassium fluosilicate 30kg, tin fluoborate 35kg, diethyl triamine 4kg, tetraethylenepentamine 1kg.
Preparation method: with embodiment 1
Embodiment 5
The anti-oxidation reducing agent raw material is formed: glutaric acid 20kg, decanedioic acid 1kg, adipic acid 1kg, zinc fluosilicate 27kg, fluosilicic acid tin 50kg, tetraethylenepentamine 1kg.
Preparation method: with embodiment 1
Embodiment 6
The anti-oxidation reducing agent raw material is formed: suberic acid 17kg, adipic acid 2kg, potassium fluoborate 35.5kg, potassium fluosilicate 43kg, triethyl group tetramine 2.5kg
Preparation method: with embodiment 2
Embodiment 7
The anti-oxidation reducing agent raw material is formed: decanedioic acid 10kg, suberic acid 19kg, zinc fluoroborate 42kg, zinc fluosilicate 24.5kg, diethyl triamine 4.5kg.
Preparation method: with embodiment 3
Embodiment 8
The anti-oxidation reducing agent raw material is formed: adipic acid 20kg, glutaric acid 4kg, potassium fluoborate 25kg, sodium tetraborate 48kg, triethyl group tetramine 3kg.
Preparation method: with embodiment 3
Now key characteristic oxygen-proof property, percent reduction, the proportion of goods damageds of the embodiment of the invention are carried out certification test in order to following method.
Oxygen-proof property: get lead-free solder 2kg, put into the automatic constant-temperature tin pot of diameter 10cm, be warming up to 260 ℃, simultaneously the 3g anti-oxidation reducing agent evenly is sprinkling upon the tin liquor surface, stir tin liquor 1min with the little spoon of stainless steel.Stir once each 1min later on every 2h.Test duration 8h skims the standard that oxidizing slag is weighed as oxygen-proof property.
Percent reduction: the oxidation scruff that will scrape from the tin pot is placed in the crucible, together puts into 700 ℃ high temperature again, and 30min is burnt in baking, takes out to be cooled to room temperature and to pour grinding scruff in the mortar into.Get thin shape oxidation tin ash 2g wherein again, put into the little spoon of stainless steel, add the 0.5g anti-oxidation reducing agent, then spoon is placed on 255 ℃-265 ℃ tin liquor surface, heat on one side and shake little spoonful, when treating that tin ash is reduced into spherical tin, stop to heat.Take out the tin ball and be placed on flush away residue dirt in the ethanol, carry out weighing, and be calculated as follows out percent reduction:
In the formula: W
1---the weight of oxidation tin ash.
W
2---be reduced into the weight of tin ball.
The proportion of goods damageds: get lead-free solder 2kg, put into the automatic constant-temperature tin pot of diameter 10cm, be warming up to 260 ℃, simultaneously the 3g anti-oxidation reducing agent evenly is sprinkling upon the tin liquor surface, stir tin liquor 1min with the little spoon of stainless steel.Stir once each 1min later on every 8h.Measure the surplus of anti-oxidation reducing agent after the test duration 72h, and calculate the proportion of goods damageds of anti-oxidation reducing agent with following formula:
In the formula: G---surplus behind the anti-oxidation reducing agent use 72h.
Result of the test sees the following form:
Test data in the last table shows that the present invention compares with existing like product, has outstanding effect aspect the anti-oxidation percent reduction of critical index, the proportion of goods damageds.Cigarette is little in the use, and the wiring board that does not have after bad smell welds is clean, is the product of high comprehensive performance.
Claims (6)
1. a molten state lead-free welding flux anti-oxidation reducing agent is the pulvis of being made by raw material reducing agent, antioxidant and dispersion promoter, and its parts by weight of raw materials proportioning is: reducing agent 8-30, antioxidant 65-90 disperses promoter 1-5.
2. reducing agent according to claim 1 is characterized in that: described reducing agent is glutaric acid, adipic acid, suberic acid, decanedioic acid, can choose wherein a kind of, two or more composite wantonly; Proportioning arbitrarily between the reducing agent of composite two or more.
3. reducing agent according to claim 1 is characterized in that: described antioxidant is potassium fluoborate, zinc fluoroborate, tin fluoborate, potassium fluosilicate, zinc fluosilicate, fluosilicic acid tin, sodium tetraborate, can choose wherein two kinds composite wantonly; Proportioning arbitrarily between two kinds of composite antioxidants.
4. reducing agent according to claim 1 is characterized in that: described dispersion promoter is diethylenetriamines, trien, tetren, optional one or both composite.Composite two kinds are disperseed between promoter proportioning arbitrarily.
5. method for preparing the described molten state lead-free welding flux anti-oxidation reduced powder of claim 1 may further comprise the steps:
A, component takes by weighing above-mentioned various raw material by weight;
B, elder generation put into rustless steel container to the reducing agent that weighs up, and are heated to and all are fused into liquid, and temperature is remained between 100-155 ℃;
C, the antioxidant that weighs up is slowly at the uniform velocity joined in the liquid of b step preparation while stirring, stop heating after in said temperature, stirring 20-30min;
The material of c step preparation is stirred in d, continuation, when its temperature drops to 30-40 ℃, adds while stirring and disperses promoter, stirs 0.5-1h again and promptly gets product of the present invention.
6. method according to claim 5 is characterized in that: in step c, mixing speed is 40-60n/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910210874A CN101693315A (en) | 2009-11-12 | 2009-11-12 | Molten state lead-free welding flux anti-oxidation reducing agent and preparation process thereof |
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| CN200910210874A CN101693315A (en) | 2009-11-12 | 2009-11-12 | Molten state lead-free welding flux anti-oxidation reducing agent and preparation process thereof |
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| CN101693315A true CN101693315A (en) | 2010-04-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528330A (en) * | 2012-01-12 | 2012-07-04 | 李平荣 | Molten solder anti-oxidation activated powder |
| CN103031453A (en) * | 2012-11-28 | 2013-04-10 | 李平荣 | Smoke-free reduction powder and anti-oxidation method thereof |
-
2009
- 2009-11-12 CN CN200910210874A patent/CN101693315A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102528330A (en) * | 2012-01-12 | 2012-07-04 | 李平荣 | Molten solder anti-oxidation activated powder |
| CN102528330B (en) * | 2012-01-12 | 2013-12-25 | 李平荣 | Molten solder anti-oxidation activated powder |
| CN103031453A (en) * | 2012-11-28 | 2013-04-10 | 李平荣 | Smoke-free reduction powder and anti-oxidation method thereof |
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